Water Systems for Personal

Care Products;

How to Meet Microbiological

Quality Requirements

Phil Greaves
BiotiQ Consulting
 Slide 2

Introduction

Water is our most important resource

No water = No life

In personal care product manufacturing

No water = No product (with a few exceptions!)

Contaminated water = contaminated product

 Slide 3

How we use Water in our Factories

• Sanitary uses

• Fire suppression
• Drinking water
• Heating and cooling – LTHW, Chilled Water

• Feedwater to other water systems – softened water, deionised water, RO

• Process cleaning & sanitization – CIP, COP
• Raw material
 Slide 4

Scope of Today’s Training

1. Water quality requirements

2. Water treatment & purification
3. Water storage
4. Water distribution
5. Microbiological control methods
6. Microbiological monitoring best practices
 Slide 5

Water Quality Requirements

Do personal care products require water of a higher

quality than drinking water?
 Slide 6

Water Quality Requirements

YES!:
• To ensure consistent quality (drinking water quality is outside our control
and can be variable)

BUT:
• Increasing the quality of water increases the cost … we have to balance
water quality against product requirements
• Chemical & physical qualities of water driven by product chemistry
requirements
• Microbiological quality of water driven by product preservation capacity
and (sometimes) health authorities
 Slide 7

Typical Examples of Water Qualities

Manufacturing Application Minimum Water Grade

Raw material - Medical devices
Raw material – Personal Care
Products
Cleaning / rinsing of product residues
Sanitization of production equipment /
lines
Same microbiological quality as water
Rinsing of sanitization chemicals
Pharmacopoeial Purified Water
DI or potable* water with enhanced
microbiological control
Potable* water with enhanced
microbiological control
Potable* water with enhanced
microbiological control
used to make product

* Potable water = City water = Drinking water

 Slide 8

Measuring Water Quality

Subjective Measures (Organoleptic properties):

• Taste, appearance, smell

Chemical / Physical Measures:

• Presence / levels of specific chemicals e.g. aluminium, heavy metals
• Conductivity
• Total Dissolved Solids (TDS)
• Total organic carbon (TOC)

Microbiological Measures:
• Total viable count (TVC)
• Specific pathogens
• Indirect measures e.g. ATP
 Slide 9

Typical Examples of Water Qualities

Water Grade Microbiological Specification Physico-Chemical Specification

Target Maximum
Total organic carbon: NMT 500 ppb
< 100 CFU / 100 Conductivity: NMT 4.3 µS / cm @ 20°C
EP Purified Water < 100 CFU / mL
mL Nitrates: < 0.2 ppm
Heavy metals: < 0.1 ppm
WHO specifications:
Conductivity: NMT 250 µS / cm @ 25°C
Potable Water with enhanced
< 200 CFU / mL < 500 CFU / mL pH: 6.5-8.0
microbiological control
Hardness: < 60 mg / L
Total dissolved solids: < 300 mg / L

CFU = Colony Forming Units

TOC = Total Organic Carbon
NMT = Not more than
WHO = World Health Organization
 Slide 10

Water Treatment / Purification

The challenge - what we have to achieve:

• Purifying water to consistently achieve our required chemical and
microbial quality

• Maintaining chemical, and especially microbial quality during purification,

storage, distribution and use

• We have to achieve this despite often very variable quality of water

delivered to our manufacturing sites
– Municipal water
– Borehole / well
– River / lake
 Slide 11

Water Treatment / Purification Processes

Water Grade Treatment / Purification Method

 Deionisation
USP / EP Purified Water
 Reverse osmosis
 Filtration (sand or membrane filters)
Potable Water  Activated carbon filter
 Softener
 Slide 12

Deionisation

• Also known as ion exchange or demineralisation

• Process removes almost all mineral ions

– Cations e.g. sodium, calcium, iron, copper
– Anions e.g. chloride, sulfate

• Replaces these ions with hydrogen (H+) and hydroxide (OH-) ions
 Slide 13

Deionisation
 Slide 14

Chemical Deionisation

• Water is based through ion exchange resin beds

– Mixed bed deioniser combines cation and anion resins in same bed
– Twin bed deionisers have separate resin beds and water passes first
through cation then into anion bed

• Regeneration of beds is necessary when ion is exhausted (cannot trap

any more ions)
• Achieved by passing strong base and/or acid solution through resin beds.
Replaces the trapped ions to allow new cycle of ion exchange
 Slide 15

Chemical Deionisation

Advantages:
• Cheap technology
• Long established technology

Disadvantages:
• Requires regular maintenance for regeneration
• Regeneration chemicals are highly corrosive – strong acid and alkali
• Limit purification capability
 Slide 16

Electro-Deionisation Technologies

• Chemically regenerated deionisation systems replaced by electro de-

ionisation – EDI
• Sometimes termed CDI – continuous or capacative deionisation

• Reduces / eliminates the need for strong acid and base regeneration,
significantly reduces system ‘down-time’
 Slide 17

Electro-Deionisation (EDI)

• Combines ion-exchange resins with ion-selective membranes with direct

electrical current to remove ionic species from water

• Ion exchange process removes ions from water by replacement with OH -

and H+ ions. Water passes through series of chambers containing ion
exchange resins held between cation and anion selective membranes
 Slide 18

Electro-Deionisation (EDI)

• Ions bind to the ion exchange

membrane and migrate to a
separate chamber due to an
applied electrical field
• This also produces OH- and H+
ions by electrolysis which are
necessary to maintain the resins
in a regenerated state
• Ion exchange beds are
continuously regenerated
 Slide 19

Electro-Deionisation (EDI)

Advantages:
• Removes dissolved ions to 5-17 MΩ /cm, TOC <20 ppb
• No chemical required for regenerating resin
• No resin or chemical disposal
•
Restrictions:
• Removes only a restricted number of charges particles, cannot produce
ultra-pure water
• Typically needs reverse osmosis treated water
 Slide 20

Electro-Deionisation (EDI) – typical packaged units

• Elga IonPro series

• 0.3 to 1.0 M3 / Hour

• UK ~ £80 - £100,000
 Slide 21

Electro-Deionisation (EDI) – typical packaged units

• Elga Orion series

• 0.5 to 5 M3 / hr

• UK ~ £150,000
 Slide 22

Reverse Osmosis

• Normal osmotic flow from low

solute to high solute
concentration is REVERSED by
applying pressure across a
semi-permeable membrane
• Not a membrane ‘sieving’ action
– mechanism is diffusion and
depends on solute
concentration, pressure and
water flow rate
 Slide 23

Reverse Osmosis

• Achieves high purity water

• High range of outputs – 10 Lt
to 50 M3 / hour
• Low energy cost (especially
compared to distillation)
• Prone to biofouling
• Pre-treatment required
 Slide 24

Reverse Osmosis

Biofouling case study

Pre-treatment is essential for any

water purification system!
 Slide 25

Pre-Treatment

• Coarse Filtration
– Sand bed filter
– 25µm membrane filter

• Activated Carbon Filter

– Reduces organic chemicals

• Water Softener
– Captures calcium and magnesium ions (replacing with sodium / salt
ions) to reduce water hardness
 Slide 26

Typical Water Treatment Plant

 Slide 27

Typical Water Treatment Plant

 Slide 28

Who’s Thirsty?

Let’s Take a Break!

 Slide 29

Water Storage

• Water must be stored in bulk such that microbial contamination and

growth is prevented (or limited to very low levels)
• Storage capacity must balance expected demand …. Transit time for
water in storage tank should be < 24 hours
• Tank should have domed top to ensure condensation does not collect
• Sprayballs fitted to water inflow from purification and water loop return
 Slide 30

Water Storage

Storage tank should be vertical not horizontal to minimize headspace

Can a sprayball reach all the

headspace surfaces in this tank?
 Slide 31

Water Storage

• Water level in tank detected by level or

weight sensors – not by sightglass or
float

• Air entry into the tank protected by

heated filter:
– Filter must prevent ingress of
bacteria (0.2µm)
– Heat prevents the build up of
condensation on the filter surface
• Condensation can allow bacteria
to grow
• Condensation reduces rate of air
entry into the vessel risking
collapse under vacuum
 Slide 32

Water Distribution

The BIG requirement is to prevent bacteria

attaching to surfaces and forming biofilm
 Slide 33

Biofilm

• In natural environments, relatively few

bacteria (and fungi) occur as free
swimming (planktonic) organisms
• Micro-organisms prefer to attach to
substrates – offers protection from being
swept away
• Colonies can develop that are complex
communities of several interacting species
– a natural phenomenon called biofilm
• Secrete extracellular lipopolysaccharide
(slime) which protects the colony
 Slide 34

Biofilm Formation
 Slide 35

Biofilm Risk Factors

• Water that has been, or is periodically, stagnant

– Distribution systems that are ‘one-way’ and do not recirculate
– Areas that cannot be drained adequately for maintenance or shut-downs
– Deadlegs
• In-line filters in distribution system
• Water systems that have poor materials of construction
– Plastic / galvanised pipes (microscopically rough surfaces)
– Poor welds (internal pits)
• Components that have surfaces that cannot be properly sanitized
– Screw threaded joints
– Ball valves
• Systems where water temperature is between 20 - 40º C

If any of the above conditions exist, there is a risk that biofilm may be present,
even if routine sampling does not detect viable organisms
 Slide 36

Detecting & Treating Biofilm

• Biofilm is not easily detected by routine micro testing of water; samples only
‘see’ planktonic (free-floating) bacteria
• Indicators of biofilm are:
– Periodic high ‘spikes’ in micro results
 Slide 37

Detecting & Treating Biofilm

• High ATP (energy molecule of living cells) where this is measured

• Open the pipework – does it feel slimy to the touch or can brown residues
be seen? (this could also be rouge = iron deposits)
• SWAB the pipework internally
Treatment:
• Preferred method is hot (60⁰C) peractic acid at > 800 ppm for at least 30
minutes (Cl2 less effective)
• Several ‘rounds’ of treatment may be necessary to remove stubborn
biofilm
• Physical disassembly and manual scrubbing with peractic acid may be
required
• Pre-treatment with protease enzyme can help
 Slide 38

Distribution System Requirements

• Water system design must follow good hygienic design principles:

• Smooth, orbitally welded 316 stainless steel
• Butterfly or diaphragm valves – no ball valves
• Sloped to drain points so the system is dry when shut-down for
maintenance: 1:100 or 3⁰ fall
• Connections made using hygienic flange connectors, not screw-thread

• Early stages of water treatment may not have or need all of these design
features
 Slide 39

Preventing Contamination – Pipework Standards

• All distribution lines constructed from 316 stainless steel

• Non-corrosive, able to resist chlorine-based disinfection
• Internal surfaces very smooth / electropolished to reduce bacterial
adhesion
 Slide 40

Distribution System Requirements

• Hygienic welds – prevent ‘pits’ for bacteria to hide in

• Orbital welding where possible
• Welds inspected
• Weld filler of the same metallurgical quality – 316 stainless steel
 Slide 41

Distribution System Requirements – Turbulent Flow

• Turbulent flow reduces possibility for bacterial attachment to pipe walls

Achieved by:
• Continuous recirculation of water
• Combination of pipe diameter and water velocity – Reynold’s number of > 12,500
• ‘Deadlegs’ e.g. to valves less than 6 times pipe diameter (can be engineered to
much less than this)
• Residence time in holding vessel – compromise between capacity and usage rate
 Slide 42

Distribution System – GOLDEN REQUIREMENTS

• Water circulation pump must be on 24 hours / 365 days year –

continuously recirculating

• Flexible pipes at water outlets:

• Cut to minimum length – NOT COILED!
• Disconnected when not in use and stored drained (inverted U-shape)
• Best practice – different colour flexible hose for each shift and replaced
/ sanitized at the end of each shift

• Accurate and up-to-date Process & Instrumentation Drawing (P&ID) for

the system
 Slide 43

What is a P&ID?
 Slide 44

THIS is a P&ID!
 Slide 45

Water Distribution System Horror Show

 Slide 46

Water Distribution System Horror Show

← Pitting in internal pipework welds

↓ Growth from a swab – Burkholderia cepacia
 Slide 47

Preventing Contamination – Bioburden Control

• Bacteria will always be present in incoming water and have the opportunity
to grow in pre-treatment and treatment systems
• We need to reduce the numbers to very low levels through bioburden
control:
– Chlorination
– UV
– Heat
– Ozone

• Remember … filtration is a poor method of bioburden control as the filter

can act as a site for biofilm formation
 Slide 48

Preventing Contamination – Water Treatment Processes

Chlorination
• Water is continuously dosed with sodium hypochlorite or chlorine dioxide
• Disassociates at correct pH range to give free available chlorine
• Very effective at killing bacteria and fungi (but not protozoa)

• Requires 1.5 ppm to be fully effective

• Water pH must be within 5.5 to 8.0 for available chlorine to be produced
• Dosing level should be linked to flow rate to give ratio control of chlorine
levels
• Requires in-line monitoring and alarming
• Remember – chlorine levels will drop to sub-lethal concentrations in
deadlegs!
 Slide 49

Preventing Contamination – Water Treatment Processes

Ultra-violet:
• In-line UV lamp with energy output above 35 mW.sec/cm2
• Requires continuous monitoring and alarming of output
• Efficiency depends on transit time (time cell is exposed to UV)
• Efficiency reduced by particles > 2.5 µm in the water – requires in-line
filtration immediately upstream of the UV
• Typically ~ 90% efficient (kills 90% of bacteria) on single pass – relies on
several pass of water over the lamp
• Problems may arise at periods of peak demand where recirculation drops
• Ineffective against biofilm – only works in one place!
• Efficiency at killing protozoa is much reduced (less good for Legionella
protection)
 Slide 50

Preventing Contamination – Water Treatment Processes

Heat:
• Water maintained continuously above 60°C or
• Water treated for 2 minutes above 80°C immediately prior to use
(Pasteruization)
• Water treated for > 20 minutes above 70°C at weekends
• Very effective but energetically expensive

Ozone:
• Relatively new technique
• Very efficient at killing bacteria – and penetrates / kills biofilm
• Typically applied at 0.1 to 0.3 ppm
• May affect product quality – requires UV lamp or heat at point of use to destroy
ozone
 Slide 51

Ozonation – Day Time Operation

Ozone Generator

Storage
Vessel

User Valves

Ultra Violet Ozone

Destruction Lamp

Pump
 Slide 52

Ozonation – Night Time Operation

Ozone Generator

Storage
Vessel

User Valves

Ultra Violet Ozone

Destruction Lamp
TURNED OFF

Pump
 Slide 53
Ozonation – Night Time Operation with user valves
opened

Ozone Generator

Storage
Vessel

User Valves

Ultra Violet Ozone

Destruction Lamp
TURNED OFF

Pump
 Slide 54

Bioburden Control Methods – Pros and Cons

Method Pros Cons Comments

Chlorination • Low cost • Residual chlorine in Only suitable for limited
• Good at preventing biofilm water can affect products e.g.
• Continuous product colour / odour / toothpastes
• Treats whole system stability
UV • Low cost • Only kills bacteria Best used with another
• Reliable passing through the UV control method e.g.
• Continuous – does not kill bacteria heat or chemical
downstream sanitization
• Risk of biofilm
Heat • Reliable technology • Expensive Dying out due to cost
• Effective at reducing biofilm • Carbon footprint and environmental
• Not continuous impact
• Safety risk – hot
surfaces
Ozone • Effective biofilm control • Initial investment The future!
• Continuous • Risk of residual ozone
• Low running costs in products
 Slide 55

Preventing Contamination – Water Treatment Processes

IF our routine water treatment process is reliable and robust, it should not be
necessary to perform additional processes to treat biofilm

BUT we may need a periodic biofilm treatment process if we have less than
perfect conditions (poor pipework, deadlegs etc):
– Typically performed every 6 months (trend analysis of micro results
useful in determining the frequency)
– Chemical dosing with peracetic acid at > 800 ppm for 30 minutes
followed by flushing with clean water
 Slide 56

Microbial Monitoring of Water Quality

“We only see what we look for”

• Microbial testing does not detect all organisms that may be present
• Increasing understanding of biofilm and difficulties of detection
– Organisms are not uniformly distributed
– Samples may not be representative
• Repeat sampling for Out Of Specification (OOS) results not possible
 Slide 57

Microbial Monitoring of Water Quality

Assurance (confidence!) in water quality comes through:

Validation:
- Intensive testing programme for new water systems and modifications to
existing systems

Routine Monitoring:
- Sampling plans that focus on key locations in purification, storage and
distribution
- At least two critical locations: Mixer user point and loop return
 Slide 58

Microbial Monitoring of Water Quality

• Performance Qualification / Process Validation

– Intensive testing period
– Key purification stages
– All user points daily for at least 4 week period
– Key / most representative locations identified

– Ongoing testing at critical for 12 months (during production use) to

determine seasonal variations
 Slide 59

Microbial Monitoring of Water Quality

• Routine Monitoring:

• Each day that water is used as raw material

• At least weekly for user points (e.g. mixers)
• At least monthly for all sample points

• TRENDING of data is more important than ‘daily’ results

– Low variability over period of time between tests indicates good control
– High variability may indicate biofilm
– Rising trend indicates loss of control
 Slide 60

Microbial Monitoring of Water Quality

Micro Test Methods:

• At least 100ml sampled at each sample location into a sterile container
• 100ml tested by membrane filtration (best practice)
• 1ml tested by pour plate method
• May be useful to do both on same sample (in-case too many bacteria
present to count in the 100ml sample)
• Agar used should be R2A agar – a low nutrient agar that mimics
conditions in water system
• Incubated for at least 3 days at 32 - 35⁰ C
– Try incubating for 7 days periodically; does the count rise?
• Trend analysis of results
 Slide 61

Microbial Monitoring of Water Quality

Beware of the ‘Pass / Fail’ trap!

• Micro monitoring of water is not about meeting a TVC / numerical limit

• It should be about understanding system performance, risks to product and
changes
• TREND is more important than actual count
• SPECIES are more important than actual count
– Need to build history and awareness of what species are routinely present
and when these change
– Need to perform species identification of colonies even when under
specification limit
LOW count of Pseudomonas or Burkholderia much greater risk than higher count
of some other bactreia
 Slide 62

Case Study

• Site in the UK
• Cold and hot water distribution systems
• Hot water has a ‘dial-in’ temperature capability by mixing hot and cold
water
• Water from purification plant is good quality with typically 0 CFU / ml
• Micro samples frequently exceed 100 CFU / ml at some locations in
distribution
• High risk Pseudomonas and Burkholderia bacteria detected
 Slide 63

Case Study – Risk Factors

Poor quality
pipework welds

Manifolds; Three way

reduced water mixing valves for
flow = temperature
insufficient control =
turbulence periodic
stagnant water
Biofilm visible
inside pipe
 Slide 64

Case Study – The Solutions

• Improve chemical sanitization by measuring peracetic acid concentration

at end of pipe / at end of contact time
• Replace distribution pipework to improve weld quality
• Redesign hot water system

Recovering from a contaminated

water situation is a lot more
expensive than designing and
installing correctly in the first place!
 Slide 65

And Finally …. The Uncontrolled Sources

Uncontrolled buckets – Poor hose management – Water dispensed into IBC’s e.g. for
often used for external trapped water filling line washout
cleaning or pig washing
Do not exceed 8 hours!
Label with contents and expiry time
 Slide 66

Water Systems for Personal Care Products

Thank You & Questions?

Philip Greaves
BiotiQ Consulting